CN104655787B - Arrowband spiral chromatographic sheet and preparation method thereof - Google Patents
Arrowband spiral chromatographic sheet and preparation method thereof Download PDFInfo
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- CN104655787B CN104655787B CN201510038743.2A CN201510038743A CN104655787B CN 104655787 B CN104655787 B CN 104655787B CN 201510038743 A CN201510038743 A CN 201510038743A CN 104655787 B CN104655787 B CN 104655787B
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Abstract
The invention provides a kind of arrowband spiral chromatographic sheet and preparation method thereof, described arrowband spiral chromatographic sheet includes substrate, the groove of zigzag shape is offered in described substrate side, the initiating terminal of described groove is at the geometric center of substrate, being provided with fixing phase in groove, described arrowband spiral chromatographic sheet not only increases development distance, and when mixture is separated, the difference of Rf value between mixture can be increased under the influence of centrifugal force, thus improve separation efficiency.
Description
Technical field
The present invention relates to analytical chemistry field, particularly to a kind of arrowband spiral thin layer color
Spectrum plate and preparation method thereof.
Background technology
Thin layer chromatography occurs in 1938 the earliest, N.A.Izmailor and
The M.S.Schraiber alumina flake trace of coating on microscope slide first
Annulus technology has separated the composition in various plants tincture.
The 1950's, J.G.Kirchner and J.M.Miller etc. was at the base of said method
Using silica gel as adsorbent on plinth, Gypsum Fibrosum Preparatum is that adhesive coated is made in glass support plate
Become silica gel thin-layer, had successfully been isolated volatile oil, thus developed thin layer chromatography.
Hereafter, E.Stahl to the standardization of thin layer chromatography, standardize and expand application
The aspects such as scope have carried out extensive work, and nineteen sixty-five, E.Stahl published " thin layer chromatography
Handbook ", make thin layer chromatography reach its maturity, extensively weighed in analytical chemistry field from this
Depending on and commonly use.
Thin layer chromatography is an important branch in chromatographic technique, and its advantage is letter
Height single, rapid, sensitive, separation efficiency are good, and can concurrently separate multiple sample,
Analysis cost is low, and the pretreatment to sample is simple, selects fixing phase and developing solvent
Degree of freedom is big, it is adaptable to containing being difficult to from separating medium desorption or containing suspended particulates
Sample analysis.
At present, thin layer chromatography be widely used in the qualitative detection such as target substance,
The detection of compound purity, quantitative analysis, organic compound synthesis tracking and monitoring, medicine
The many aspects such as thing analysis and assay, in qualitative, sxemiquantitative and quantitative analysis
In play an important role.
Although thin layer chromatography is a kind of efficient in terms of separating given material different component,
Cheap and effective method, but close in separation complicated (such as phospholipid etc.) or retention
Mixture time, the length of chromatographic sheet just receives certain restriction, i.e. in exhibition
Open apart from interior, it is impossible to the component in mixture is separated one by one, and straight line increases distance
Not solution problem method because separating degree only be proportional to open up away from square root.
And in the case of point sample is the least, increase over time, can not avoid thin
After layer chromatography separates, speckle spreads the situation causing separating degree to reduce, and result is not easy to see
Examine, can be to calculating RfValue causes difficulty.
Rotary thin layer, also known as centrifugal thin layer, is in thin layer, centrifugal paper chromatography and column chromatography
The circular TLC separation of the continuous eluting of a kind of centrifugal type grown up on the basis of Deng
Technology, due to apparatus structure be simple and convenient to operate, the advantage such as good separating effect,
It is widely used in the preparative separation of synthesis and natural product.
Its development history can trace back to the thirties in 20th century, has people centrifugal force for dividing
From to reduce destruction, beneficially boiling point is high, the separation of molecular weight large compound, the sixties
Dalcortivo et al. separates alkalescence poisonous substance with accelerating centrifugal paper chromatography, obtains satisfied knot
Really.
The separation principle of rotary thin layer is dug up the roots according to sample between fixing phase and flowing mutually
Absorption, distributional effects difference outside, add the effect of centrifugal acceleration, make sample
In original R between each componentfValue (Rf value) difference strengthens, thus improves point
From effect, accelerate separating rate.
Though rotary thin layer chromatograph relies on the effect of centrifugal acceleration, make each component RfValue difference
Different increasing, improves separation, but can not avoid the sample point diffusion after separating,
The qualitative and quantitative analysis of sample is added difficulty.
Therefore, needing a kind of horizontal proliferation of exploitation badly little, development distance is big, separation efficiency
High chromatographic sheet.
Summary of the invention
In order to solve the problems referred to above, present inventor has performed and study with keen determination, found that:
On substrate, with the geometric center of described substrate as starting point, offer the recessed of zigzag shape
Groove, arranges fixing phase in groove, and prepared chromatosheet not only significantly increases expansion
Distance, and limit sample horizontal proliferation on chromatosheet, described chromatosheet exists
Use under centrifugal condition, play the effect of pressured column chromatograph, improve Rf value difference
The little separation efficiency between component, thus complete the present invention.
It is an object of the invention to provide following aspect:
First aspect, the present invention provides a kind of arrowband spiral chromatographic sheet, its feature
Being, described chromatosheet includes substrate, offers the groove of zigzag shape on substrate,
Fixing phase it is provided with in described groove.
Second aspect, the present invention also provides for one and prepares above-mentioned arrowband spiral thin layer chromatography
Method, it is characterised in that said method comprising the steps of:
(1) with the geometric center of substrate as starting point, in substrate side, to substrate limit
Edge offers the groove of zigzag shape；
(2) fixing phase grinding is become powder；
(3) powder that step 2 obtains is mixed with dispersion liquid, form mix homogeneously
Suspension；
(4) suspension that step 3 prepares is fed to the groove of substrate, remove and divide
After dissipating liquid, i.e. obtain arrowband spiral chromatographic sheet.
Accompanying drawing explanation
Fig. 1 illustrates that embodiment 1 prepares arrowband spiral chromatographic sheet photo；
Fig. 2 illustrates that embodiment 2 prepares arrowband spiral chromatographic sheet photo；
Fig. 3 illustrates that embodiment 3 prepares arrowband spiral chromatographic sheet photo；
After Fig. 4 illustrates experimental example 1 separation component, arrowband spiral chromatographic sheet shines
Sheet, wherein,
A is the mottle of methylene blue；
B is the mottle of rhodamine B；
After Fig. 5 illustrates experimental example 2 separation component, arrowband spiral chromatographic sheet shines
Sheet, wherein,
A is the mottle of methylene blue；
B is phenol red mottle.
Drawing reference numeral explanation
1-through hole
Detailed description of the invention
Below by the present invention is described in detail, the features and advantages of the invention will
Become more apparent from, clearly along with these explanations.
The most special word " exemplary " means " as example, embodiment or explanation
Property ".Here as any embodiment illustrated by " exemplary " should not necessarily be construed as being better than or
It is better than other embodiments.Although the various aspects of embodiment shown in the drawings, but
It it is unless otherwise indicated, it is not necessary to accompanying drawing drawn to scale.
The present invention described below.
According to the first aspect of the invention, it is provided that a kind of arrowband spiral chromatographic sheet,
It is characterized in that, described chromatosheet includes substrate, offers zigzag shape on substrate
Groove, described groove is provided with fixing phase.
Substrate of the present invention, preferably regular polygon or circle, as square,
Regular hexagon, octagon or circle, more preferably circle.
The material of described substrate is the thin layer chromatography base of any one material in prior art
Plate, such as glass plate, metallic plate or polyvinyl chloride panel etc..
It is highly preferred that substrate even density, thickness is uniform.
In the present invention, described helix is involute helix, preferably hyperbolic spiral shell
Line, logatithmic spiral and Archimedes spiral etc., its function under polar coordinate is once
Function, quadratic function or exponential function etc..
At the geometric center that the initiating terminal of the groove of described zigzag shape is on substrate,
It extends along zigzag shape on substrate, and preferably end extends to substrate edges, described
Groove is by initiating terminal to end, and width keeps constant；Described groove is by initiating terminal extremely end
End, the degree of depth keeps constant.
The most only offer a groove, be used for preparing arrowband spiral thin layer color
Spectrum plate.
The size of described groove is not specially limited by the present invention, preferably the width of groove
It is 0.5～5.0mm, more preferably 1.0～4.0mm, deep such as 3.0mm, preferably groove
Degree is 1.0～3.5mm, and preferably 1.5～4.0mm, such as 2.0mm.
In a preferred embodiment of the invention, the width of groove initiating terminal is more than
The width of groove, it is preferable that the width of the width ratio groove of groove initiating terminal is big
10～11mm, consequently facilitating the developing solvent added is fixed and is fully absorbed mutually and permeate,
Sample to be separated is divided by the enough developing solvents of fixing middle absorption mutually making arrowband helix chromatography
From.In further preferred embodiment, groove initiating terminal is circular, described
The circular diameter bigger than the width of groove 10～11mm at top, to be separated on groove
Sample the most easily launches along groove direction in fixing mutually.
Any one of described fixing prior art of use mutually is for preparing thin layer chromatography
Fixing phase, preferably silica gel G, silica gel G F254, silica gel H, silica gel H F, aluminium oxide,
Zirconium oxide, Hydro-Giene (Water Science)., lanthanum fluoride, silver iodide, barium fluoride, calcium fluoride, simple substance
Sulfur, Silver monobromide and zinc sulfide etc., more preferably barium fluoride and silica gel G, the most excellent
Electing silica gel G as, silica gel G absorption property height, Heat stability is good, stable chemical nature are also
And there is higher mechanical strength.
Described arrowband spiral chromatographic sheet can be same using polyvinyl chloride panel as substrate
Time, using silica gel G as fixing phase；Can also be using metallic plate as substrate, meanwhile,
Using barium fluoride as fixing phase；Can also be using polyvinyl chloride panel as substrate, with fluorination
Barium is as fixing phase；Can also be using metallic plate as substrate, meanwhile, with silica gel G F254
As fixing phase.
The inventors discovered that, the granularity of fixing phase is the least, and component to be separated is at chromatosheet
On development distance difference the biggest, separating effect is the best, but when the granularity of fixing phase is little
When 50nm, component to be separated resistance when fixing middle expansion mutually increases, and causes separating
Speed substantially reduces, even, and the component to be separated horizontal proliferation speed in fixing mutually
More than its deployment rate, and then causing separating effect to reduce, therefore, the present invention selects
The granularity of described fixing phase is 50nm～40 μm, preferably 80nm～10 μm, more preferably
100nm～800nm.
In a preferred embodiment, substrate is not offered the position of groove,
Can offer through hole 1, described through hole 1 is along being perpendicular to substrate surface direction, for by base
Plate is fixed on chromato fuge.
Preferably, substrate offers one or more through hole 1, preferably 2.
According to the second aspect of the invention, also providing for one, to prepare above-mentioned arrowband spiral thin
The method of layer chromatography, it is characterised in that said method comprising the steps of:
Step 1, with the geometric center of substrate as starting point, in substrate side, to substrate
The spiral yarn shaped groove of edge.
Step 2, becomes powder by fixing phase grinding.
The inventors discovered that, the granularity of fixing phase is the least, and component to be separated is at chromatosheet
On development distance difference the biggest, separating effect is the best, but when the granularity of fixing phase is little
When 50nm, component to be separated resistance when fixing middle expansion mutually increases, and causes separating
Speed substantially reduces, even, and the component to be separated horizontal proliferation speed in fixing mutually
More than its deployment rate, and then separating effect is caused to reduce, therefore, person of the present invention
The granularity selecting fixing phase is 50nm～40 μm, preferably 80nm～10 μm, more preferably
100nm～800nm.
Fixing described in step 2 is to fix phase described in first aspect mutually.
Step 3, powder step 2 obtained mixes with dispersion liquid, forms mix homogeneously
Suspension.
The inventors discovered that, be dispersed in fixing mutually in dispersion liquid, form suspension,
Suspension is laid in described groove, after removing dispersion liquid, shape in described groove
Become is dried fixing phase, uniformly, closely, good separating effect.
What that prepare used by chromatographic sheet in prior art dispersion liquid of the present invention be
Meaning a kind of dispersion liquid, preferably water and/or ethanol.
The powder that step 2 is obtained by the present invention does not do limit especially with the weight ratio of dispersion liquid
Fixed, it is possible to the powder making step 2 obtain fully infiltrates in dispersion liquid, form mobility
Good solidliquid mixture is preferably, such as the weight of the powder that step 2 obtains: dispersion liquid
Weight=1:(5～20), preferably 1:(8～15), such as 1:10.
The mode that the powder that step 2 is obtained by the present invention mixes with dispersion liquid is not done especially
Limit, be uniformly dispersed as preferably in dispersion liquid with the powder that step 1 can be made to obtain,
As ultrasonic wave added mixes, mechanical agitation mixing etc..
Step 4, in suspension charging step 3 prepared to the groove of substrate, removes
After dispersion liquid, i.e. obtain arrowband spiral chromatographic sheet.
The method removing dispersion liquid is also not specially limited by the present invention, recessed not destroy
Pattern and the performance of fixing phase in groove are preferred, as dispersion liquid can be by volatilizing naturally
Method remove, it is also possible to heating under conditions of remove.
For using, water sensitive is fixed the arrowband spiral chromatographic sheet prepared mutually,
Can at high temperature activate before use.
The arrowband spiral chromatographic sheet its preparation method provided according to the present invention, has
Following beneficial effect:
(1) development distance under unit are is added by spiral curve；
(2) rely on centrifugal acceleration effect make development distance no longer as common thin layer that
Sample is restricted, and makes the forward position of developing solvent constantly to advance；
(3) curvilinear equation under helix is at polar coordinate along substrate upper groove determines
After, by regulation rotating speed to change angular velocity omega, control the size of its centrifugal acceleration,
Thus be conducive to promoting moving ahead of developing solvent；
(4) improve the thickness of narrow band thin-layer chromatographic sheet by deepening depth of groove, can carry
High point sample number of times, is additionally, since chromatosheet narrow width, in the restriction of groove two side
Under, the horizontal proliferation of sample is effectively suppressed；
(5) sample is after narrow band thin-layer chromatographic sheet is launched to separate, horizontal due to sample
Diffusion is suppressed, thus sample integrated distribution；
(6) fixing phase consumption is few, significantly reduces cost；
(7) method preparing described arrowband spiral chromatographic sheet is simple, it is easy to operation.
Embodiment
Embodiment 1
(1) on the circular lamellae of polrvinyl chloride, it is initial at its place, center of circle
It is linear function (Archimedes spiral, f (θ)=2 θ) that point offers the f (θ) extended to edge
Groove, recess width is 3mm, the degree of depth is about 2mm；
(2) 0.7g barium fluoride nano-particle is joined in mortar, be fully ground,
Particle diameter to barium fluoride nano-particle is about 95nm；
(3) prepare addition 10mL ethanol in powder to step 2, proceed to the title of 30 × 60
In measuring bottle, ultrasonic 20min, form suspension, after standing 2min,
(4) aspiration step 3 obtains upper suspension, from the beginning of groove initiating terminal, all
In the even groove spreading upon polrvinyl chloride lamellae, make fixing phase surface even uniform,
Place at horizontal level, treat that ethanol volatilizees, fixing near doing of turning white mutually, prepare surface and put down
Whole arrowband spiral chromatographic sheet, as shown in Figure 1.
Embodiment 2
(1) on the circular lamellae of polrvinyl chloride, it is initial at its place, center of circle
It is linear function (Archimedes spiral, f (θ)=2 θ) that point offers the f (θ) extended to edge
Groove, recess width is 3mm, the degree of depth is about 2mm；
(2) take 10g silica gel G (400 mesh), be placed in beaker；
(3) to equipped with the 50g that adds water in the beaker of silica gel G, mix homogeneously, sheet is placed
Carve, until bubble-free is emerged in suspension；
(4) suspension after mixing, from the beginning of groove initiating terminal, uniform application are drawn
In the groove offered on polrvinyl chloride chromatosheet, make fixing phase surface even uniform,
Place at horizontal level, treat that water volatilizees, fixing near doing of turning white mutually, prepare surfacing
Arrowband spiral chromatographic sheet, as shown in Figure 2.
Embodiment 3
(1) on the circular lamellae of polrvinyl chloride, for rising at its place, center of circle
It is exponential function (logatithmic spiral, f (θ)=e that initial point offers the f (θ) extended to edge0.2θ)
Groove, recess width is 3mm, the degree of depth is about 2mm；
(2) take 10g silica gel G (40 μm), be placed in beaker；
(3) to equipped with the about 50g that adds water in the beaker of silica gel G, mix homogeneously, place
For a moment, until in suspension bubble-free emerge；
(4) suspension after mixing, from the beginning of groove initiating terminal, uniform application are drawn
In the groove offered on polrvinyl chloride chromatosheet, make fixing phase surface even uniform,
Place at horizontal level, treat that water volatilizees, fixing near doing of turning white mutually, prepare surfacing
Arrowband spiral chromatographic sheet, as shown in Figure 3.
Experimental example
Experimental example 1 separates rhodamine B and methylene blue
Experimental technique:
Weigh 0.02g rhodamine B and 0.02g methylene blue respectively in weighing botle, respectively
Add 10ml dehydrated alcohol, be configured to the rhodamine B sterling solution and 0.2% of 0.2%
The sterling solution of methylene blue；Mix by its volume ratio 1:1 during use.
Rhodamine B by 0.2% and the biased sample point of the methylene blue of 0.2% away from
At spiraled narrow strip chromatograph starting point 15～18mm, developing solvent is dimethyl sulfoxide,
Launch under 2550rpm rotating speed.
As shown in Figure 4, wherein, A is time first to arrowband spiral chromatographic sheet after separation
The mottle that base is blue, B is the mottle of rhodamine B.
As shown in Figure 4, after spiraled narrow strip development of chromatogram separates, rhodamine B and time first
Base indigo plant is kept completely separate.
Experimental example 2 separates phenol red and methylene blue
By phenol red ethanol solution (concentration is 0.5%) and methylene blue, (concentration is
0.2%) mixing for 1:1 by volume, biased sample point is away from spiraled narrow strip color
At spectrum starting point 15～18mm, developing solvent is dimethyl sulfoxide, at 2800rpm rotating speed
Under launch.
As it is shown in figure 5, wherein, a is time first to arrowband spiral chromatographic sheet after separation
The mottle that base is blue, b is phenol red mottle.
As shown in Figure 5, after spiraled narrow strip development of chromatogram separates, phenol red and methylene blue
It is kept completely separate.
Above in association with detailed description of the invention and exemplary example, the present invention is carried out in detail
Illustrate, but these explanations can not be interpreted as limitation of the present invention.This area skill
Art personnel understand, without departing from the spirit and scope of the invention, and can be to this
Inventive technique scheme and embodiment thereof carry out multiple equivalencing, modify or improve,
These are within the scope of the present invention.Protection scope of the present invention is wanted with appended right
Ask and be as the criterion.
Claims (12)
1. an arrowband spiral chromatographic sheet, it is characterised in that described chromatosheet bag
Include substrate, substrate offers groove and the through hole (1) of zigzag shape, described
Being provided with fixing phase in groove, the width of described groove is 0.5～5.0mm, and the degree of depth is
1.0～3.5mm；
Described helix is hyperbolic conchoid, logatithmic spiral and Archimedes spiral；
The initiating terminal of described groove is at the geometric center of substrate；
Described groove extends along zigzag shape on substrate；
Described groove is by initiating terminal to end, and width keeps constant；With
Described groove is by initiating terminal to end, and the degree of depth keeps constant.
Arrowband the most according to claim 1 spiral chromatographic sheet, its feature exists
In, the width of described groove is 1.0～4.0mm.
Arrowband the most according to claim 2 spiral chromatographic sheet, its feature exists
In, the width of described groove is 3.0mm.
Arrowband the most according to claim 1 spiral chromatographic sheet, its feature exists
In, the degree of depth of described groove is 1.5～3.5mm.
Arrowband the most according to claim 4 spiral chromatographic sheet, its feature exists
In, the degree of depth of described groove is 2.0mm.
Arrowband the most according to claim 1 spiral chromatographic sheet, its feature exists
In, described fixing mutually selected from silica gel G, silica gel G F254, silica gel H, silica gel H F, oxygen
Change aluminum, zirconium oxide, Hydro-Giene (Water Science)., lanthanum fluoride, silver iodide, barium fluoride, calcium fluoride,
Elemental sulfur, Silver monobromide and zinc sulfide.
7. prepare one of claim 1～6 described arrowband spiral chromatographic sheet for one kind
Method, it is characterised in that said method comprising the steps of:
(1) with the geometric center of substrate as starting point, in substrate side, to substrate limit
Edge offers the groove of zigzag shape；
(2) fixing phase grinding becoming particle diameter is 50nm～the powder of 40 μm；
(3) powder that step 2 obtains is mixed with dispersion liquid, dispersion liquid be water and/
Or ethanol, form the suspension of mix homogeneously；
(4) suspension that step 3 prepares is fed to the groove of substrate, remove and divide
After dissipating liquid, i.e. obtain arrowband spiral chromatographic sheet.
Method the most according to claim 7, it is characterised in that in step 2, will
Fixing phase grinding becomes particle diameter to be 80nm～10 μm.
Method the most according to claim 8, it is characterised in that in step 2, will
The powder that fixing phase grinding becomes particle diameter to be 100nm～800nm.
Method the most according to claim 7, it is characterised in that in step 3,
The powder that step 2 obtains and the weight that weight ratio is the powder that step 2 obtains of dispersion liquid:
Weight=the 1:(5～20 of dispersion liquid).
11. methods according to claim 10, it is characterised in that in step 3,
The powder that step 2 obtains and the weight that weight ratio is the powder that step 2 obtains of dispersion liquid:
Weight=the 1:(8～15 of dispersion liquid).
12. methods according to claim 11, it is characterised in that in step 3,
The powder that step 2 obtains and the weight that weight ratio is the powder that step 2 obtains of dispersion liquid:
Weight=the 1:10 of dispersion liquid.
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| US3538744A (en) * | 1967-11-09 | 1970-11-10 | Phillips Petroleum Co | Chromatography apparatus |
| NL8105758A (en) * | 1981-12-21 | 1983-07-18 | Univ Leiden | Sepn. by radial thin layer chromatography - supplying eluant centrally on to plate with absorbent clamped on rotating carrier |
| CN2924532Y (en) * | 2006-07-17 | 2007-07-18 | 长沙川戈科技发展有限公司 | Rod thin layer chromatograph |
| US9164068B2 (en) * | 2009-07-01 | 2015-10-20 | Brigham Young University | Thin layer chromatography plates and related methods |
| CN102707012B (en) * | 2012-05-11 | 2014-12-24 | 北京大学 | Narrow band thin-layer chromatographic sheet and preparation method thereof |
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